高等学校化学学报

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稀土(镧)硫醇盐的合成与表征

祝纶宇1,2, 许凯1, 王洪1,2, 刘鹏1,2, 陈德宏1,2, 艾好1,2, 陈鸣才1   

    1. 中国科学院广州化学研究所, 广东省电子有机聚合物重点实验室, 广州 510650;
    2. 中国科学院研究生院, 北京 100049
  • 收稿日期:2007-11-23 修回日期:1900-01-01 出版日期:2008-09-10 发布日期:2008-09-10
  • 通讯作者: 陈鸣才

Synthesis and Characterization of Rare Earth(Lanthanum) Thiolate

ZHU Lun-Yu1,2, XU Kai2, WANG Hong1,2, LIU Peng1,2, CHEN De-Hong1,2, AI Hao1,2, CHEN Ming-Cai1*   

    1. Key Laboratory of Polymer for Electronics of Guandong Province, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650, China;
    2. Graduate School of the Chinese Academy of Sciences, Beijing 100049, China
  • Received:2007-11-23 Revised:1900-01-01 Online:2008-09-10 Published:2008-09-10
  • Contact: CHEN Ming-Cai

摘要: 以三氧化二镧为原料, 经过醇化, 制备了三(月桂硫醇)镧及三(巯基乙酸异辛酯)镧, 并对合成方法进行了优化. 采用热失重分析、FTIR光谱、感应耦合等离子色谱、元素分析和1H NMR对目标产物进行了表征. 确定合成稀土异丙醇盐最佳反应条件为: 反应温度80 ℃, 反应时间2 h; 合成三(月桂硫醇)镧的反应条件为反应温度110 ℃, 反应时间2 h, 月桂硫醇的摩尔分数过量24%; 合成三(巯基乙酸异辛酯)镧的反应条件为反应温度60 ℃, 反应时间2 h, 月桂硫醇过量32%.

关键词: 硫醇盐, 镧, 巯基乙酸异辛酯, 月桂硫醇

Abstract: Rare earth thiolates, lanthanum tri(isooctyl thioglycolate) and lanthanum tri(dodecyl thiolate), were prepared from lanthanum oxide by utilizing exchange reaction of rare earth alkoxide. The products were characterized via TGA, FTIR, 1H NMR, ICP and element analysis. The optimization of synthesis condition was made. The optimal synthesis condition of lanthanum isopropoxide is at the temperature of 80 ℃ for 2 h; the optimal synthesis condition of lanthanum tri(dodecyl thiolate) is at the temperature of 110 ℃ for 2 h and the dodecyl thiol overdoses by 24%; and The optimal synthesis condition of lanthanum tri(isooctyl thioglycolate) is at the temperature of 60 ℃ for 2 h and the isooctyl thioglycolate overdoses by 32%.

Key words: Thiolate, Lanthanum, Isooctyl thioglycolate, Dodecyl thiol

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